Citation: QIN Zhan-Jie, ZHANG Xiang-Ru, PENG Zhang-Kuang, LI Qing-Kuan, MA Yun-Qi, FAN Qi-Shun, DU Yong-Sheng, WANG Jian-Ping, SHAN Fa-Shou. Extraction and Separation of Boron in Anhydrite and Gypsum Minerals and Its Isotopic Measurement by Thermal Ionization Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(1): 48-54. doi: 10.11895/j.issn.0253-3820.170331
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The anhydrite and gypsum are the main sulfate minerals during evaporation of seawater or lake. They record the information about relative hydrogeology and the composition of mother liquor. Boron is diffluent element, and often occurs in all kinds of evaporites. Presently, the boron isotope has been applied widely in mineral deposits forming, geochemistry and palaeoenvironment. However, there is little research about characteristic of boron isotope in anhydrite and gypsum minerals, because of the low content of boron and micro-solubility in water and hydrochloric acid. This study developed a method of extracting and purifying boron in anhydrite and gypsum by phase transformation and ion-exchange. Firstly, the samples were mixed with ammonium hydrogen carbonate to transform the calcium sulfate to calcium carbonate. And diluted hydrochloric acid (1 mol/L) was added to resolve calcium carbonate. The percent conversion was about 85% in the first stage, and up to complete resolution by repeating this process. Secondly, boron specific ion-exchange resin (Amberlite IRA 743) was used to gather the boron ions fully and further refined the samples with more than 1 μg of boron by anionic and cationic resin mixed by Ion Exchange Ⅱ and Dowex 50 W×8. Finally, according to the modified method by He, the values of boron isotope were determined by TIMS. The boron content is analytically pure gypsum was 3.501±0.128 μg/g (n=12, RSD=3.6%) and the average recovery was 100.47%. Besides, the δ11B value of analytically pure gypsum added with NIST SRM 951 was 17.98‰±0.21‰ (n=3, RSD=1.2%). This method has good repeatability and can meet the requirements of boron isotopic measurement of anhydrite and gypsum.
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